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TMR-AQUA BOND 0

Product Report～An adhesive that has realized rapid treatment
under moist conditions～

YAMAKIN CO., LTD.

Head Office: 3-7 Sanadayama-cho Tennoji-ku Osaka 543-0015, Japan
Biological Science Safety Laboratory:
Laboratory in the Department of Oral and Maxillofacial Surgery, Kochi Medical School, Kochi University
Kohasu, Oko-cho, Nankoku-shi, Kochi 783-8505, JAPANBranch Office: Tokyo, Osaka, Sendai, Nagoya, Fukuoka, JAPAN
P: +81-887-55-0281 F: +81-887-55-0053
E: contact@yamakin-gold.co.jp

EditedEdited by
by YAMAKIN
YAMAKIN Ph.D.
Ph.D. GroupGroup

https://www.yamakin-global.com
INTERNATIONAL20201022

Index
1. Introduction ・・・・・・・・・・・・・・・・・・・・・・・・・ 2
2. Development background ・・・・・・・・・・・・・・・・・ 3
2.1 Adhesive focusing on moisture ・・・・・・・・・・・・・・・・・・・・ 3
2.2 Challenges for the development of TMR – AQUA BOND 0 ・・・・・・・・・ 5
2.3 Functions of “TMR-AQUA BOND 0” as realized ・・・・・・・・・・・・・ 5
3. Adhesion to tooth substance ・・・・・・・・・・・・・・・・ 6
3.1 Evaluation of the initial adhesive strength to tooth substance ・・・・・・・・ 6
3.2 Evaluation of adhesion under moist conditions ・・・・・・・・・・・・・・ 7
3.3 Adhesion per demineralization time ・・・・・・・・・・・・・・・・・ 8
4. Adhesion to materials other than tooth substance ・・・・ 9
4.1 Adhesion to zirconia ・・・・・・・・・・・・・・・・・・・・・・・ 9
4.2 Adherends other than zirconia not requiring primer ・・・・・・・・・・・・ 10
4.3 Adherend requiring the combined use of primer ・・・・・・・・・・・・・ 12
5. Adhesion process ・・・・・・・・・・・・・・・・・・・・・・ 12
6. Retention of uniformity ・・・・・・・・・・・・・・・・・・・ 14
7. Adhesive interface ・・・・・・・・・・・・・・・・・・・・・・ 15
8. TMR series・・・・・・・・・・・・・・・・・・・・・・・・・・ 16
9. Biological safety ・・・・・・・・・・・・・・・・・・・・・・・ 18
10. Conclusion ・・・・・・・・・・・・・・・・・・・・・・・・・ 20
Supervision
YAMAKIN Ph.D. Group
Teruo Anraku (Ph.D. in Engineering)
Hiroyuki Itoigawa (Ph.D. in Science)
Takahiro Kato (Ph.D. in Engineering)Takeshi Sakamoto (Ph.D. in Pharmacy)
Yuji Sato (Ph.D. in enterpreneur engineering)
Hidekazu Tanaka (Ph.D. in Engineering)
Ritaro Matsuura (Ph.D. in Agriculture)
Masatoshi Yamazoe (Ph.D. in Dentistry)
Hirohisa Yamamoto(Ph.D. in entrepreneur engineering)
Advisor of YAMAKIN Ph.D. Group
Bunichiro Yamada (Ph.D. in Engineering)
What is the YAMAKIN Ph.D. Group?
This is a group of experts in various specialized fields who combine their knowledge, experience andtechnical expertise to act as a prime mover in the continuous generation of innovation.

TMR-AQUA BOND 0 Product Report
Kato, T., Ph.D. in Engineering, Executive Officer, Head Researcher, Development Department
Matsuura, R., Ph.D. in Agriculture, Senior Chief Researcher, Biological Science and Safety Laboratory
Sakamoto, T., Ph.D. in Pharmacology, Chief Researcher, Organic Material Development Section
Mizuta, Y., Master of Engineering, Project Leader, Organic Material Development Section
Hayashi, M., Master of Agriculture, Biological Science and Safety Laboratory

1. Introduction
It can be said that dental adhesives have grown along with the evolution of composite resin (CR)restoration.

YAMAKIN developed an adhesive designed for convenience of use and ability to adhere to materials
other than tooth substance. "TMR-AQUA BOND 0" (AQUA BOND) was successfully developed byapplying the comprehensively usable "Multi Primer" 2, 3) technology derived from YAMAKIN’s basic
research and "iGOS BOND" 4) technology, which has high adhesive strength and adhesion resistant to themoist conditions in the oral cavity.
"AQUA BOND" is an adhesive which has both adequate strength and bonding durability to eachadherend, even when demineralization time and photoirradiation time are shortened. This is acombination which had been difficult to realize before.
In this report, we will discuss the performance of "AQUA BOND" as along with its actual verification
results. We hope that you will be interested in "AQUA BOND" as a highly reproducible adhesive that canmeet the demand of clinical treatment by achieving adhesion that can tolerate a wide range of adhesion
conditions, and as a product that can reduce complications and treatment time.

In particular, CR restoration has spread rapidly as a highly effective treatment method of repair for
dental caries 1) due to the MI (Minimal Intervention) approach to treatment. MI was proposed in 2000 asa way to minimize the area of intervention in the infected tooth, and to leave as much sound tooth as
possible in place.

2. Development background

The CR which fills in the minimum cavity has almost no adhesion to the tooth substance. Therefore, aspecialized adhesive between CR and tooth is required. When such an adhesive first appeared, it was of a
3-liquid type, in line with the adhesion process adopted (priming, permeating and bonding to the tooth).
Subsequently, the adhesive was simplified to a 2-liquid or 1-liquid type by the introduction of afunctional compounds such as adhesive monomers, which are effective for organic chemistry andhigh-polymer chemistry. Also, sufficient a strength and durability have been realized even with 1 liquid
type adhesive by this technique. Furthermore, as an interesting example, CRs that do not requireadhesives are beginning to be developed, but it can be said that there is still room for further study on
their physical properties.

2.1 Adhesive focusing on moisture
We develop adhesives, focusing on the moisture involved in dental adhesion.
“The moisture involved in adhesion” refers to a wide range of phenomena, such as moisture entering
during cavity formation, tissue fluid that seeps out of the dentinal tubule of dentin, to capillary action
and osmotic pressure on the adhesive interface, water vapor contained in exhalation, and the water
introduced when removing the adhesive material solvent by air-blowing 5).

In view of the above circumstances, the development of adhesives in the future will proceed primarily bysimplifying the method of adhesion and expanding the adherend.
"Simplifying the method of adhesion" includes reducing or shortening of the steps required for adhesion;for example, the wait time (decalcifying time) until the surface is etched after application of the adhesiveto the tooth substance, or shortening the time required forvisible light irradiation (light irradiation time) in thesubsequent curing.
“An adhesive with an expanded range of adherends” refers
to a product that can be used not only for dentin but also formaterials such as precious metals, non-precious metals andceramics. Adhesives that can adhere to these materials
without primers have already been put on the market.
In the development of such technology, strength andbonding durability to the above materials have become
issues; efforts to resolve these issues have been made, butthere is remaining room for improvement.

―2―

TMR-AQUA BOND 0"AQUA BOND" is created from accumulation of YAMAKIN's unique adhesive technology. We will
explain the technical background of its creation.

For adhesion, a minimum amount of moisture is necessary for wettability and permeability to theadhesive interface; however, such a minimum amount of moisture will cause disproportionation anddilution of the adhesive composition and lead to adhesion failure. Also, since the latter inhibiting factor
greatly affects the outcome in clinical cases, adhesion is done with attention paid to moisture-proofing
measures.
However, in clinical cases of moisture-proofing, it is difficult to prevent moisture penetrating fromvarious routes.
For example, in adhesion of dentin, when an adhesive is applied to treated dentin surface, it is thought that
osmotic pressure causes the interstitial fluid to leak from the dentinal tubule to the interface. It is very
difficult to prevent moisture from penetrating into this adhesive, and there are many uncertainties as tohow much moisture permeates an area of cavity and to what extent it becomes a hindrance to adhesion 6).
Since components of adhesive include hydrophobic organic compounds such as crosslinking monomers,
it is thought that water enters from outside and water is localized in the phase separation of thecomposition or in the vicinity of the interface between the adhesive and the tooth. In such a situation,
moisture gathers in the vicinity of the interface, and an adhesive layer which is fragile with respect toadhesion is formed. Furthermore, water drops in the vicinity of the interface may wash out monomers
from the adhesive layer. Especially in the case of acidic monomers, they will continue to scrape the tooth―3―

surfaces even after curing; as a result, the weakened adhesive interface may cause detachment from theadherend 6).
In order to prevent the possibility of deterioration of adhesion due to such phase separation, it is possible
to prevent phase separation of the composition with a surfactant or the like. However, since ordinary
surfactants have no polymerizability, they essentially do not take part in a curing reaction byphotopolymerization, but rather they cause a reduction in strength when they are applied in large
amounts; therefore, it is necessary to pay attention to the formulation.
Therefore, YAMAKIN has planned the development of an adhesive from a new perspective.
In other words, from the idea of "making moisture work for us," we have devised an adhesive in such a
way that adhesion is not susceptible to being affected by moisture which cannot be excluded clinically(Figure 1).
Positive Influences

Negative Influences

Adhesive mechanism

Influence on material•Mediation of tooth demineralization action•Deterioration during storage(Hydrolysis of monomers)•Activation of acidic monomer•Integration or transport of calcium salt

Influence on bond durability•Deterioration of surface of adhesive(Hydrolysis of cured item)

Interface•Improvement of wettability of adherend
surface•Wash effect on pollutant•Deterioration of surface of adhesive(Washing out of residual monomer)

making moisture workfor us

2.2 Challenges for the development of TMR-AQUA BOND 0
In this way, we were able to develop an adhesive with good reproducibility in adhesion under a moist
conditions. However, against a background of increasingly simplified processes and shortened treatment
times in dental adhesion, there was growing demand for products which did not require leaving time(demineralization time) after application, and which could adhere not only to dentin but also toprosthetic appliances. Our conventional product adhered to dentin with good reproducibility, but it did
not allow for shortening of demineralization time or adhesion to prosthesis without primer.
The development challenges for "AQUA BOND" were shortening demineralization time and lightirradiation time (polymerization time), increasing the number of adherends, and maintaining highadhesive strength and durability so that we could provide a product to users who wanted to simplify
adhesion processes and shorten treatment time. Therefore, M-TEG-P was essential as a functionalmonomer to realize "AQUA BOND".
2.3 Functions of “TMR-AQUA BOND 0” as realized"AQUA BOND" can adhere to various adherends without a primer, as given in the following table. With
"Multi Primer LIQUID" (Multi Primer), it can adhere to porcelain and resin materials containing
inorganic fillers (resin material). AQUA BOND was designed to be used in combination with resinmaterial and porcelain in combination with primer. This is because we determined that the maintenanceof storage stability and adhesion durability could be compromised if silane coupling agent (which
imparts adhesiveness to both materials) is concentrated with strongly acidic monomer into one liquid.
Therefore, the need for primer has not been completely eliminated.

Influence on adhesion•Unevenness of adhesive•Adhesion failure due to adherent getting
mixed with contaminants such as saliva andmilling dust during adhesion operation

Table 1 Adherends of AQUA BOND (With/without combined use of primer)
TMR-AQUA BOND 0

TMR-AQUA BOND 0＋
Multi Primer LIQUID

Tooth substance✓ー

Zirconia✓−

Titanium✓−Gold alloy✓−

Silver alloy✓−

Gold-silver-palladium alloy✓−

Resin (inorganic fillers)−✓

Porcelain−✓

Product nameFigure 1 Positive and negative influences on "making moisture work for us" in adhesion
First, in the composition of an adhesive, we focused on adhesive monomers and developed an originaladhesive. In this process, we succeeded in developing M-TEG-P® phosphate monomer and introducing it
into the composition of dental adhesive "iGOS BOND" (“our conventional product”). Thanks to
M-TEG-P, we have succeeded in developing an adhesive whose components will not exhibit phaseseparation during the solvent volatilization that occur after application, and whose adhesion will not besusceptible to influence by the amount of moisture mixed into the adhesive layer.
M-TEG-P is a registered trademark of YAMAKIN CO., LTD.

Adherend

O
O

O

O

O

O

Polymerizing group

Tetraethyleneglycol part

O

P

OH

OH

Phosphate group

Characteristic properties•Demineralization effect by phosphate group can be controlled by organic group.
•Higher detergency than phosphoric acid
•Improvement of wettability

Figure 2 Chemical structure and characteristics of M-TEG-P
By "making moisture work for us," we were able to create a product that is tolerant to conditions such as amoist adherend environment, to air-blowing conditions after application, or leaving time (underlight-shielded) after removing it from the container and which can adhere with good reproducibility.

―4―

For shortening treatment time, AQUA-BOND enables the next step of the process to be performed
during the decalcifying time: solvent removal by air-blow immediately after an adhesive is applied on an
adherend, including tooth substance. During light irradiation time, as long as the LED lamp has a lightamount of 1000 mW/cm2 or more, AQUA-BOND can be cured and adhere well with good reproducibility
with irradiation of 10 seconds or more without any particular additional requirements. Furthermore, inthe case of LED lamps with a light amount of 2400 mW/cm2 or more, adhesion by irradiation for 3
seconds or longer can be reliably achieved.
Figure 3 shows a list of initial adhesive strengths of each material. For resin material and porcelainmaterial, adhesion with combined use of "Multi Primer" together is evaluated. Detailed evaluation
methods of adhesion will be described later.

―5―

3.2 Evaluation of adhesion under moist conditions
The oral cavity is a high-humidity environment, and there are circumstances where dry the tooth surface
cannot be dried sufficiently during cavity formation, or where moisture cannot be prevented even if due
care is taken. Therefore, adhesion of "AQUA BOND" in a moist condition was evaluated. In thisevaluation method, after adherend surface was dried, the tooth surface was moistened uniformly so as tobe covered with a thin film of water, and then the adhesive strength was examined as a model evaluation.

Tensile bond strength (MPa)

30
25
20
15
10

Test specimens for adhesion test in a dry condition and a moist condition are shown in Figure 5.

50

BovineenamelFigure 3

BovinedentineZirconia

TitaniumGold alloy

Silver alloy

Gold-silverpalladium alloy

Resin block
Porcelain(with(with Multi primer)
Multi primer)

Initial adhesive strength to tooth substance and to each of the other materials above

3. Adhesion to tooth substance

3.1 Evaluation of the initial adhesive strength to tooth substance
Adhesion to tooth substance of "AQUA BOND" is evaluated with bovine teeth. Evaluation was carriedout with the test method shown in Figure 4.
The following outline is of a test of modeling composite restoration in the oral cavity. Masking tape witha 3-mm diameter hole was affixed on each polished flat surface of bovine enamel and bovine dentine tolimit the adhesive surface. After the adherend surface was dried by air-blowing, "AQUA BOND" wasapplied. Five seconds after application (demineralization time), the applied surface was dried byair-blowing and polymerized by light. After that, the composite resin for dental filling was filled andcured. A stainless steel rod was fixed to this cured surface using resin cement to prepare a test specimen.
The specimen was stored in water at 37 °C for one day and then subjected to a test to pull the stainlesssteel rod perpendicularly to the adherend surface at a speed of 1 mm/min, and the tensile bond strength
was obtained from stress at breaking.
Bovine Investment

Polishing (P600)/ Air-blowing
after cleaning

Masking with Φ3 mm

TMR-AQUA BOND 0
Applying and air-blowing

Preliminary polymerization

dry condition

In a moist conditions, "AQUA BOND" is applied and bonding is carried out in a state where a film ofwater of about 100 μm covers the tooth surface. The results are shown in Figure 6.
"AQUA BOND" showed effective adhesion to both enamel and dentin even when it was adhered undermoist conditions. It is thought that due to the effect of M-TEG-P, wettability to the tooth surface of thewhole composition is effective under both dry and moist conditions and the maintenance of adherence
uniformity realizes highly reproducible adhesion under both dry and moist conditions.

Fillingcomposite resin

Setting a transparent film
and pressure

Photopolymerization

dry condition

16

moist condition

14
12
10
8
6
4
2
0

Installation of O ringmoist condition

Figure 5 Test specimens for adhesion test (dry condition and moist condition)

Tensile bond strength (MPa)The evaluation of adhesion of "AQUA BOND" was carried out as follows. The relationship between
demineralization time and adhesion of "AQUA BOND" was evaluated, as was adhesion in a moist model.

EnamelDentinFigure 6 Adhesion to tooth substance (dry conditions, moist conditions)Removing film and applying
resin cement

Fixing a jig fortensile test

Tensile test after storingfor one day

Figure 4 Method of adhesion to tooth substance

―6―

―7―

3.3 Adhesion per demineralization time
"AQUA BOND" is designed to maintain high adhesion even if the demineralization time and lightirradiation time after application are shortened in order to reduce the burden on the patient. The
demineralization time after application and the adhesion of "AQUA BOND" were confirmed. It was thenconfirmed whether there was a cause-and-effect relation between them depending on the time. The
adhesion to the tooth substance at different demineralization times is given in Figure 7.
"AQUA BOND" did not desorb enamel or dentin even under any of the demineralization time conditions,and in comparison with our conventional product, stronger adhesion was confirmed, especially undershorter demineralization time conditions for enamel. By contrast, for dentin, it can be seen that there isno notable decrease of adhesion even with relatively long demineralization for 20 seconds. This showsthat the reaction between M-TEG-P and hydroxyapatite on the surface of the tooth is moderately
controlled. That is, M-TEG-P efficiently removes the smear layer on the surface of the enamel anddentin, or the calcium component as the smear plug, and forms a preferable surface for adhesion.
Therefore, "AQUA BOND" can adhere immediately after application; adhesiveness gently increases withtime due to controlled demineralization, and it has been demonstrated dhesion will not decrease due toexcessive demineralization etc. in dentin.

TMR-AQUA BOND 0

16

Our conventional productTensile bond strength (MPa)Tensile bond strength (MPa)In other words, "AQUA BOND" can be said to be tolerant to demineralization time rather than not
requiring demineralization time.

14
12
10
8
6
4
2
0

0

10

20

TMR-AQUA BOND 0

16

Our conventional product

14
12
10
8
6
4
2
0

0

10

Demineralization time (sec)

Demineralization time (sec)

EnamelDentine20

4. Adhesion to materials other than tooth substanceMaterials other than tooth substance, zirconia, titanium and precious alloys can be adhered without
primer. Especially of interest is the adhesion to zirconia.
Here, we will discuss adhesion to materials other than tooth substance. The materials used as adherends
are as given in Table 2.
Table 2 Materials used as adherends
Material

Product name

Zirconia

KZR-CAD Zr SHT

Titanium

KZR-CAD Ti

Gold alloy

YP GOLD TYPE I

Silver alloy

UNI 1-nGold-silver-palladium alloy

PALLAZ 12-n

Resin block

KZR-CAD HR Block 3 GAMMATHETA

Porcelain

ZEO CE LIGHT

4.1 Adhesion to zirconia
Regarding adhesion characteristic to zirconia, adhesive strength was evaluated with "KZR-CAD Zirconia
SHT" ceramics for dental machining. The evaluation was carried out by the test method given in Figure
8. The outline of the test method is as follows and is a modeling test assuming repair in the oral cavity.
Masking tape with a hole of 3 mm diameter was attached to the polished flat surface of zirconia, to limit
the adhesive surface. After drying the adherend surface by air-blow, "AQUA BOND" was applied. Fiveseconds after application (leaving time), the applied surface was dried by air-blow and polymerized byirradiation of light. After that, the composite resin for dental filling was filled and cured.
A stainless steel rod was fixed on this cured surface using resin cement to prepare test specimens. The
specimens were stored in water at 37 °C for 1 day and then subjected to a test to pull the stainless steel
rod perpendicularly to the adherend surface at a speed of 1 mm/min, and the tensile bond strength was
obtained from stress at breaking.

Figure 7 Adhesion per demineralization time (Enamel and dentine)
Masking with Φ3 mm

TMR-AQUA BOND 0
Applying and air-blowing

Preliminary polymerization

Installation of O ring

Filling composite resin

Setting transparent film
and pressure

Photopolymerization

Removing film and applying
resin cement

Fixing a jig for tensile test

Tensile test after storing
for a day

Polishing (P600)/ Air-blowing
after cleaning

Figure 8 Method of adhesion to zirconia

―8―

―9―

12

Tensile bond strength (MPa)25

Tensile bond strength (MPa)

Adhesion of “AQUA BOND” to zirconia is shown in Figure 9. Even without the use of primer, "AQUA
BOND" showed stronger adhesion to zirconia than our conventional product, which is used in
combination with "Multi Primer." It is known that phosphate monomer is excellent in reactivity withzirconia 7-9) ; therefore, the phosphate group of M-TEG-P contained in "AQUA BOND" works effectively
for adhesion to zirconia. While M-TEG-P has been used as an adhesive monomer in our conventional
product, we have succeeded in preparing the composition so as to make M-TEG-P exhibit morefunctional efficiently in "AQUA BOND." Therefore, high adhesion not only to tooth substance but also tozirconia has been obtained.

20
15
10
5

10
8
6
4
2

25

20

5

TMR-AQUA BOND 0

Our conventional product(used in combination
with Multi Primer)

Figure 9 Adhesion to zirconia
4.2 Adherends other than zirconia not requiring primer
In addition to zirconia, adherends that can be adhered without primer are titanium, precious alloys, andthe like. Adhesiveness of titanium, gold alloy, silver alloy and gold-silver-palladium alloy were evaluatedusing the same method as in Figure 8, and the results are shown in Figures 10 to 13.

12

12

10

10

8
6
4
2
0

8
6
4
2
0

TMR-AQUA BOND 0 Our conventional product(used in combination
with Multi Primer)

Figure 12 Adhesion to silver alloy

TMR-AQUA BOND 0 Our conventional product(used in combination
with Multi Primer)

Figure 13 Adhesion to gold-silver-palladium alloy

In the case of adhesion to titanium which is in the same Group 4 as zirconia, our conventional productalso contains M-TEG-P, so that titanium can be adhered to without a primer; however, as with theabove-mentioned titanium and with zirconia, by adjusting the composition, an improvement inadhesiveness whereby M-TEG-P and titanium surface can interact more efficiently is observed.
Our conventional product can adhere to precious alloys by using "Multi Primer LIQUID" in combination
with it as a primer. "AQUA BOND" has components with adhesiveness to precious metals, so it canadhere to them without primer.
For adhesives containing a primer component, proximity to the adherend is hindered by the othercomponents, and the efficiency of the interaction between the primer component and the adherend is lessthan that of adhesives which require the separate use of a primer. Apart from its primer component,"AQUA BOND" is composed of similar main ingredients, including methacrylate and dimethacrylate, as
our conventional product. If we compare the two, it should be expected that the adhesion of "AQUA
BOND," which contains a primer component, will be inferior.
However, "AQUA BOND" is characterized by exhibiting higher adhesion to any precious alloy than ourconventional product used with primer.

― 10 ―TMR-AQUA BOND 0 Our conventional product(used in combination
with Multi Primer)

Figure 11 Adhesion to gold alloy

Tensile bond strength (MPa)

10

0

0

TMR-AQUA BOND 0 Our conventional product(used in combination
with Multi Primer)

Figure 10 Adhesion to titanium

15

Tensile bond strength (MPa)Tensile bond strength (MPa)0― 11 ―

4.3 Adherend requiring the combined use of primer"AQUA BOND" is designed so that it can adhere to resin material and porcelain etc. by primer treatment
with "Multi Primer LIQUID." There are two reasons for this— the problem of the efficiency of chemicalinteraction between the primer component and the adherend, and the problem of the storage stability of
the adhesive itself.
The above problems can be solved depending on the primer component used, and as described in theprevious section, "AQUA BOND" has demonstrated adhesion to a precious metal when used in
combination with adhesive components. By contrast, a silane coupling agent is effective as a primer
component for a resin material and porcelain, but since the silane coupling agent is chemically very
unstable with respect to acid and water, in blending silane coupling agent into an adhesive, it is especiallydifficult to resolve the problem of water. From these circumstances, from the viewpoint of providing astable adhesive, "AQUA BOND" was designed so as not to excessively simplify the adhesion system.
Figures 14 and 15 show the adhesion to a resin material (resin block was chosen in this report) andporcelain. In both cases, it can be seen that the adhesion system of "AQUA BOND" and "Multi Primer"
exhibits high adhesion. It can be proposed as a combination of “Multi Primer” and “AQUA BOND 0”
that can reliably adhere to new resin materials such as resin blocks, which have considerable issues inregard to adhesion.

Tensile bond strength (MPa)Tensile bond strength (MPa)

10

5

0

TMR-AQUA BOND 0

Figure 14 Adhesion to resin block

2. In the air-drying procedure, when the product is dried until the liquid surface does not move (5seconds or longer at high pressure), a uniform thin film is formed due to the characteristics of "AQUA
BOND."
3. In polymerization by light, if a thin film is uniformly formed, it will be cured by irradiation at a lightintensity of 2400 mW/cm2 for 3 seconds or longer with a light irradiator for dental polymerization.
When an adherend is a crown restoration (porcelain or resin material) for repairing in the oral cavity or
the like, it is necessary to apply "Multi Primer" for surface treatment before "AQUA BOND" application(Figure 17). The subsequent procedure is the same as the procedure for adhering to tooth substance.

Applying Multi Primer LIQUID and drying(in cases of porcelain and resin material)

Note: The drying time is in

約10秒

※2

15

10

Perform surface roughening, cleaningand drying.

5

Air-drying
TMR-AQUA BOND 0

Note: When performing
air-drying, air-blow is
performed for about 10
seconds while performing
suction with a vacuum.

Apply Multi Primer LIQUID (optional
item) on dried adherend surface anddry it for approx. 60 seconds.

Apply TMR-AQUA BOND 0 to the entire
adherend surface. After application,
air-drying can be performed even
without waiting time.

Light irradiation

Our conventional
product

Category

Fillingcomposite
resin

Figure 15 Adhesion to porcelain(used in combination with Multi Primer)

Applying TMR-AQUA BOND

約60秒※1 case of natural drying.

20

0

Our conventional
product

1. For some products, there is a need to agitate the adhesive on the applied tooth surface with anapplicator brush or the like for a certain period of time during the application procedure, in order topromote demineralization and penetration. However, with "AQUA BOND," it is enough to simply apply
the product gently on the tooth surface.

Surface roughening, cleaningand drying of adherend surface

25

15“AQUA BOND” employs a simple adhesive process with 1 step and 1 liquid. The process consists of 1)
applying, 2) Air-drying and 3) light curing, and then filling composite resin to complete (Figure 16).

(used in combination with Multi Primer)

LED light

Air-drying until the liquid surface will
not be moved while performing
suction with a vacuum.

Irradiation time

2400 mw/cm2

3 seconds or more

1200 mw/cm2
300 mw/cm2 or more

Halogen Light

5. Adhesion process

Light intensity

300 mw/cm2 or moreCuring with a light irradiator for
dental polymerization.

(for about 5 seconds or more with strongpressure)

Application

Light irradiation

Air-drying

Filling Loading
composite
resin

Apply AQUA BOND on entire driedcavity.
After application, air-drying can be
performed even without waitingtime.

Perform air-drying until the liquidsurface will not be moved while
performing suction with vacuum(for about 5 seconds or more withstrong pressure).

Category
LED light

Light intensity

Irradiation time

2400 mw/cm2

3 seconds or more

1200 mw/cm2
300 mw/cm2 or more

Halogen Light

Figure 17 Procedures for repairing dental restorations(zirconia, metal, porcelain and resin material) in the oral cavity

10 seconds or more

300 mw/cm2 or more

Figure 16 How to use AQUA BOND

― 12 ―― 13 ―

10 seconds or more

6. Retention of uniformity

7. Adhesive interface

Since M-TEG-P has stable characteristics both in water and oil, it also has the effect of maintaining ahomogeneous state without separation of the lipophilic monomer and water.

In general, minute irregularities caused by machining exist on the tooth surface in a cavity. For thisreason, adhesive needs to fill the minute irregularities and provide a smooth surface of adhesive layer toenable composite resin to adhere to the cavity surface without gaps. By contrast, in order to sufficiently
exert the physical strength of the filled composite resin, it is desirable that the thickness of the adhesive
layer, which is inferior in strength, is as thin as possible.

Therefore, as given in Figure 18, "AQUA BOND" has been confirmed to be usable without phaseseparation until about 30 minutes after removal from the container under light-shielded conditions. A
comparison of the adhesive strength of "AQUA BOND" immediately after removal with that 30 minutes
after removal is given in Figure 19. Although the adhesive strength of "AQUA BOND" to enamel
decreased by having "AQUA BOND" let sit, sufficient adhesive strength is maintained. Also, with respect
to dentin, there was hardly any change in adhesive strength. This is attributable to the fact that evenwhen the solvent component contained in "AQUA BOND" volatilizes, it does not separate, and maintains
uniformity; as a result, it shows high reproducibility of adhesion.

The adhesive interfaces between dentin and AQUA BOND and composite resin are shown in Figure 20.
It was confirmed that the interface between the adhesive layer and the composite resin was smooth,
without being affected by the unevenness of the tooth surface, and that "AQUA BOND" was able to forma smooth surface of adhesive layer. Furthermore, although the thickness of the adhesive layer depends on
the irregularities of the tooth surface, it is 5 to 10 μm, and it was also confirmed that a homogeneous thinbond layer was realized.

Composite
resin
AQUA BOND
No separation

Immediately after removal

No separation

10 min later

30 min later

Under light-shielding at 25°C

Under light-shielding at 25°C

DentinFigure 18 State immediately after removal, 10 min later and 30 min later
EnamelTensile bond strength (MPa)16

Immediately after removal
10 min later (Under light-shielding)
10 min later (Under light-shielding)

14

DentineFigure 20 Adhesive interfaces

12
10
8
6
4
2
0

EnamelDentineFigure 19 Adhesive strength immediately after removal from container,
10 min later and 30 min later― 14 ―― 15 ―

8. TMR series
In addition to "AQUA BOND", as of August 2018 the TMR series developed by YAMAKIN includes
resin-based restorative material "TMR-Z Fill 10." (Z Fill) and the dental pulp-capping material"TMR-MTA cement Mielle" (MTA cement Mielle). This is a product series that serves the mission of "noextracting," " minimal grinding" and "preserving teeth," based on the MI concept.

It is known that phosphoric acid monomer is excellent in reactivity with zirconia 7-9), so it is thought thatcombining the zirconia contained as a radiographic agent in "MTA cement Mielle" and the phosphategroup of M-TEG-P contained in "AQUA BOND" will work effectively for adhesion (Figure 23).

TMR-MTA cement Mielle

TMR-MTA cement Mielle

Figure 22 Image of interface

Figure 24 shows the evaluation results for the adhesive strength of the system (TMR series) that adheres"Z Fill" to MTA Cement using "AQUA BOND". After being mixed with water, the paste is filled into asilicone mold, and air-dried (up to 30 seconds) 5 minutes after mixing; "AQUA BOND" is applied
thereon, followed by air-drying and irradiation with light. "Z Fill (Flow)" is applied and irradiated withlight; a stainless steel rod is fixed with resin cement as a test piece, and the tensile bond strength ismeasured one day later. As shown in Figure 24, a defined range of adhesive strengths has been confirmed
by utilizing the TMR series, and it can be said that these are new values discovered in this combination.

Tensile bond strength (MPa)

Adhesive
MTA

6

4

2

0

0

10

20

Air-drying time (seconds)

MTA＋ Adhesive ＋CR＝ TMR Series

Figure 24 Adhesion by TMR series

Figure 21 Innovation through the TMR Series― 16 ―

Zirconia Fine Particles

Figure 23 Combining M-TEG-P and Zirconia

8CR

M-TEG-P

-P

M-TEG

G-P

TE

P

-P

TMR-AQUA BOND 0

GTE

EG
-T

M

Thanks to their particular functions, the following products have a range of possibilities which we intend
to pursue in the future: "MTA cement Mielle" has good sealing properties, exhibits excellent stability
after setting, and promotes hard tissue formation, as recognized in experiments and in the academic
literature, "AQUA BOND" adheres to "MTA cement Mielle" and allows CR filling immediately after thedental pulp protection achieved by "MTA cement Mielle" (the adhesion concept will be described later);,and "Z Fill" releases fluoride ions, and can be expected to strengthen tooth substance and inhibit bacteria
adhesion.
We will conduct clinical verification in the future, and we plan to report our findings at academic
conferences and in reports.

M-

M-

Let us take pulp capping as an example. Pulp capping is an important procedure to protect the pulp andpreserve the tooth. However, its success rate is low, and it is said that there are many cases in which
extraction is chosen in order to avoid subsequent risk of infection. In order to solve such process gap towhatever extent possible, YAMAKIN has developed an innovative product that includes the functionalityof the TMR series (Figure 21).

<Adhesion concept of “MTA cement Mielle” and AQUA BOND”>"MTA cement Mielle" is made into a paste by being mixed with water, and thus contains moisture. As aresult, it is not a good match for hydrophobic bonding materials. However, "AQUA BOND" ishydrophilic, and it includes M-TEG-P (which displays amphiphilic properties) as an adhesivecomponent. It is thus a good match, even though "MTA cement Mielle" contains water, and it is thoughtthat it will closely adhere to irregularities of the cement surface (Figure 22).

― 17 ―

30

The dental materials used in the oral cavity should be evaluated for any risk of adverse biological effecton the patient. This is called “biological safety evaluation”; it includes the evaluation of material risks
for cytotoxicity, irritation, sensitization, genetic toxicity and so on. This section describes the cytotoxicity
testing of "AQUA BOND" using the human monocytic leukemia cell line THP.1 cell (distributed by the
Department of Oral and Maxillofacial Surgery, Kochi Medical School, Kochi University).
The test specimen was prepared as follows. "TWiNY" was filled into a mold with a diameter of 15 mm and a
thickness of 1 mm, and then cured according to the manufacturer's instructions. Using "AQUA BOND" or
our conventional product, we adhered two layers of "TWiNY" to prepare a test specimen. A referencematerial was prepared by overlapping two layers of "TWiNY" without adhesive (Figure 25).
Test specimen

Reference material

Cells cultured on the test specimen were harvested, and then mixed with trypan blue. The number ofliving cells and dead cells in the mixture were counted with a hemocytometer. The cell viability wascalculated from the proportion of living cells to total cells.
We have reported that the reference material "TWiNY" indicated excellent biocompatibility in thistest 11). Test specimens, which include "TWiNY" and dental adhesive ("AQUA BOND" or ourconventional product), showed the equal cell viability to the reference material.
100

Cell viability (%)

9. Biological safety

80
60
40
20
0

"AQUA BOND" or our conventional productFigure 25 Test specimens for the cytotoxicity test
The test specimen was placed in a well of a 24-well plate. 100,000 THP.1 cells were seeded on thespecimen, and cultured at 37 °C under 5% CO2 for 3 days. The cultured cells were harvested andsubjected to trypan blue dye exclusion test and WST - 8 cytotoxicity test.
Trypan blue-exclusion test 10）
As shown in Figure 26, when cells are cultured on material with cytotoxicity, the cytotoxic components
destroy the cell membrane. Since cell membranes can exclude pigment compounds such as trypan blue,
dead cells, whose membranes have been destroyed, are stained blue by trypan blue. On the other hand,living cells with cell membranes are not stained with this pigment. Therefore, counting the stained cells
and non-stained cells can evaluate the effect of a test specimen on the viability of THP.1 cells.
When toxic components are eluted froma test specimen, cells are damaged andcell membranes are destroyed.

THP.1Cell

TMR-AQUA BOND 0

Our conventional
product

Reference material

Figure 27 Influence of adhesive on viability of THP.1 cell
WST-8 Cytotoxicity test 12, 13)
In the WST-8 cytotoxicity test, the indicator WST-8 has been metabolized to orange-colored WST-8
formazan by living cells. Since absorbance of WST-8 formazan is determined at 450 nm, the influence ofthe test specimen on the metabolic activity of THP.1 cells can be evaluated by the measured absorbance.
NO2

NO2

SO3-

SO3N

H
N

N
N+

SO3-

SO3-

NO2

N
MeO

Dehydrogenase

WST-8

N
N

N

NO2

MeO

WST-8 formazan

WST-8 is reduced to orange-colored WST-8 formazan by the activity of dehydrogenase in cells.
NO2

Test Specimen
Toxic components

SO3SO3-

Orange: light

H
N

N
N

NO2

N
MeO

High toxicity: Amount of WST-8 formazan
decreases due to lowering of metabolic
activity of cells.

TB

Trypan blue
Dead cell

NO2

TB
SO3-

Living cell
SO3-

Orange: dark

H
N

N
N

N

NO2

MeO

Trypan blue is taken into the cell with destroyed cell membrane, and stains the cytoplasm.

Figure 26 Principle of Trypan blue exclusion test

Low toxicity: Amount of WST-8 formazan ishigh due to continuation of metabolic activityof cells.

Figure 28 Principle of WST-8 Cytotoxicity test

― 18 ―― 19 ―

Cells cultured on a test specimen were transferred to a well of a 96-well culture plate, and WST-8 reagent
was then added to the well. After incubation at 37 °C for 2 hours, the absorbance of WST-8 formazan wasmeasured at 450 nm. The metabolic activity of THP.1 cells cultured on the test specimen, which includes“AQUA BOND” or our conventional product, was equivalent to that of the reference material (Figure 29).

References
1) Van MeerbeekB, Van Landuyt K, De munck J, Hashimoto M, Peumans M, Lambrechts P, Yoshida Y,
Inoue S, Suzuki K. Technical-sensitivity of contemporary adhesives. Dent Mater J, 24: 1, 2005.
2) YAMAKIN Ph.D. Group (Ed.): Product Report on Multi Primer Series. YAMAKIN CO., LTD., 2017.

Absorbance (450 nm)

2.53) Kimura, H, Sakamoto T, Yamada B: Noble primer composed of a silane coupling agent and multi-thiol
for adhesion of versatile dental materials, J. Appl. Polym. Sci, in press, 2018.

24) YAMAKIN Ph.D. Group (Ed.): Basic Information and product Report on Dental Bonding Material.
YAMAKIN CO., LTD., 2016.

1.5
15) Washino T, Fukunishi K, Minami M, Ishida T. (Ed.): Secchaku no shikumi to tsukaikonashi (The
Mechanism and Handling of Adhesives). QDT, 41: 54-63, 2016.

0.5
0TMR-AQUA BOND 0

Our conventional
product

Reference material

Figure 29 Influence of adhesive on metabolic activity of THP.1 cells6) Sakamoto T, Kimura H, Ohkawauchi K, Mizuta Y, Hayashi M: Chemistry of Dental Adhesives. Journalof the Adhesion Society of Japan, 52(5): 152-165, 2016.
7) Shimoe S, Hirata I, Otaku M, Matsumura H, Kato K, Satoda T: Formation of chemical bonds
onzirconia surfaces with acidic functional monomers. Journal of Oral Science, 60(2), 187-193, 2018.

As mentioned above, the reference material "TWiNY" has excellent biocompatibility 11). The addition of"AQUA BOND" or our conventional product to "TWiNY" showed no effect on the biocompatibility of"TWiNY" in the trypan blue dye exclusion test or the WST-8 cytotoxicity test. These results suggest that
"AQUA BOND" is a safe product without non-acceptable cytotoxicity for biological tissue.

8) SS Atsu, MA Kilicarslan, HC Kucukesmen, PS Aka: Effect of zirconium-oxide ceramic
surfacetreatments on the bond strength to adhesive resin. Journal of Prosthetic Dentistry, 95(6),430-436, 2006.

10. Conclusion

10) Correa GT，Veranio GA，Silva LE，Hirata Junior R，Coil JM，Scelza MF，Cytotoxicity evaluation of
two root canal sealers and a commercial calcium hydroxide paste on THP1 cell line by Trypan Blue
assay．J. Appl. Oral Sci.，17: 457-461，2009．

9) A Piwowarczyk, H-C Lauer, JA Sorensen: The shear bond strength between luting cementsand
zirconia ceramics after two pre-treatments. Operative Dentistry, 30(3), 382-388, 2005.

YAMAKIN focusses on water, which is indispensable in adhesion, and the relationship between waterand adhesive, which greatly contributes to decrease in adhesion. We have developed an adhesive that can"make moisture work for us." The presence of the amphiphilic phosphate monomer M-TEG-P is the key,and by examining the composition that makes the best use of this monomer, we have succeeded in
improving the functional efficiency of M-TEG-P. As a result, "AQUA BOND" exhibits higher adhesivestrength to tooth substance than our conventional product, even though the demineralization time andpolymerization time are shortened. For zirconia, titanium and various precious alloys, AQUA BOND canadhere even without primer, and in an adhesion system combined with Multi Primer, it can adhere withgood reproducibility to resin material and porcelain.

11) Matsuura R. Mikagi E, Horiguchi K, Anraku T. Yamamoto T: Involvement of residual monomer oncytotoxicity of resin for dental crown. Journal of the Japanese Society for Dental Materials andDevices, 29 (5): 464, 2010.

As described above, "AQUA BOND" is a material that is easy to use and can be confidently proposed as ahighly versatile adhesive. We would be pleased if you are interested in this report and use it in clinicalcases.

KZR-CAD Zr
Controlled Medical Device, Ziconia blank for dental milling and machining

The cytotoxicity test was carried out in collaborative research with the Department of Oral andMaxillofacial Surgery, Kochi Medical School, Kochi University.

12) Ishiyama M，Miyazono Y，Sasamoto K，Ohkura Y，Ueno K，A Highly Water-Soluble DisulfonatedTetrazolium Salt as a Chromogenic Indicator for NADH as Well as Cell Viability．Talanta，44:
1299-1305，1997．
13) Tominaga H，Ishiyama M，Ohseto F，Sasamoto K，Hamamoto T，Suzuki K，Watanabe M，Awater-soluble tetrazolium salt useful for colorimetric cell viability assay．Anal. Commun.，36: 47-50，
1999．

KZR-CAD Ti
Controlled Medical Device, Dental titanium non-casting alloy
YP-GOLD TYPE 1-n
Controlled Medical Device, Dental casting gold alloy
UNI 1-nControlled Medical Device, Dental casting silver alloy
PALLAZ 12-n
Controlled Medical Device, Dental casting gold-silver-palladium alloy
KZR-CAD HR Block 3 GAMMATHETA
Controlled Medical Device, Resin material for dental milling and machining
CAD/CAM Crown material for molars
ZEO CE LIGHT
Controlled Medical Device, Metal ceramics for restorations
iGOS-BOND
Controlled Medical Device, Dental adhesive for coronal dentine(Dental adhesive for dental ceramics) (Dental adhesive for dental metal)― 20 ―― 21 ―

LineupControlled medical device- Dental Adhesive for Enamel and Dentine (Dental adhesive for ceramics) (Dental adhesive for metal)

We will continue to create value for the future.

Single Package

TMR-AQUA BOND 0 (5mL)

Set Package

TMR-AQUA BOND 0 Set

Set Package

2 pcs Pack of TMR-AQUA BOND 0

Accessory

Disposable Applicator Brush : 50 pcs.
Disposable Plate : 50 pcs.

・TMR−AQUA BOND 0 (5mL)：1pc.
・Disposable Applicator Brush：50 pcs.
・Disposable Plate：25 pcs.

・TMR−AQUA BOND 0 (5mL)：2pcs.

Related Products
Controlled medical device -Resin-based Dental Restorative Material

Single Package

TMR-Z Fill10.
Universal 3.8g (2mL)

Single Package TMR-Z Fill10.

Single Package

Flow 2.6g (1.5mL)

Accessory. Needle Tip: 10 pcs.

Set Package

Standard Pack (each 1 of A1, A2, A3, E)
・Universal
A1x1
・Flow
A2x1
A3x1
・Low Flow
Enamelx1

Accessory

Needle Tip: 20 pcs.

2 pcs Pack (each 1 of A2, A3)
・Universal
A2x1
・Flow
A3x1
・Low Flow

TMR-Z Fill10.
Low Flow 2.6g (1.5mL)

Accessory. Needle Tip: 10 pcs.

3 pcs of Same Shade Pack (Each 3pcs.of A2, A3, A3.5)
・Universal
・Flow
・Low Flow

A2x3
A3x3
A3.5x3Controlled medical device - Dental pulp capping material

Single Package

Storage bag withdesiccant to prevent
moisture
Microtube Type

Glass Container / Bottle Type

Glass Container / Bottle Type

0.2gx3pcs.

3g

10g

TMR-MTA cement Mielle (White, Light Ivory)
・Microtube Type (0.2g) : 3 pcs.
TMR-MTA cement Mielle (White, Light Ivory)
・Glass Container / Bottle Type (3g)・Accessory: Spoon (1 pc.)
TMR-MTA cement Mielle (White, Light Ivory)
・Glass Container / Bottle Type (10g)・Accessory: Spoon (1 pc.)

Controlled medical device-Dental etching material (Adhesive material for dental ceramics)

Controlled medical device- Bonding material for dental metal (dental ceramics, dental resin)

Multi-use Etchant for
Various Types of Materials and Tooth

For intraoral repair of restorations(metal, ceramics and resin)

Single Package
Accessory

Multi Etchant (2mL)
Accessory : Needle tip 5 pcs.

Single Package

Multi Primer LIQUID (7mL)

Needle tips for Multi Etchant : 10 pcs.

Manufactured by

1090-3 Otani, Kamibun, Kagami-cho, Konan-shi, Kochi, 781-5451 Japan

M-TEG-P is a registered trademark of
YAMAKIN CO., LTD.
The actual color of the product, model andpackage may differ from the photographs due
to printing ink and shooting conditions.

Clean room in the YAMAKIN Kochi factory

All manufacturing processes are conducted in clean rooms and controlled extremely strictly.

《Previously Published Technical Reports》
Technical Report on ZEO CE LIGHT (Aug. 2002)
Technical Report on Luna-Wing (May 2007)
Technical Report on TWiNY ( Jul. 2010)《Previously Published Safety Test Reports》
Vol. 1 Pursuing International Standards in Quality and Safety (Dec. 2004)

Vol. 2 ZEO METAL Series Elution Test and in Vitro Cytotoxicity Test ( Jun. 2005)

Vol. 3 Elution Test and in Vitro Cytotoxicity Test of Precious-Metal Alloys and Gold Alloys for Metal Ceramic Restoration Use (Dec. 2005)
Vol. 4 Biological Evaluation of Luna-Wing ( Jun. 2006)

Vol. 5 Report on Physical Properties and Safety of High-Carat Gold Alloys (Oct. 2007)

Vol. 6 Examination of the Biological Impact of the Physical Properties of Dental-Material Alloys and Gold Alloys for Hard Resin and Metal Ceramic Restoration
Use (May 2008)

Vol. 7 Report on the Physical Properties and Safety of the Gold Alloy Nexo-Cast (Oct. 2008)
Vol. 8 Biological Evaluation of the Hybrid Composite Resin, TWiNY ( Jun. 2010)

Vol. 9 Chemical and Biological Characteristics of Precious-Metal Alloys: Elution Characteristics Produced Through Mixture with Titanium (Feb. 2011)
Vol. 10 Physical Properties and Safety of the Precious-Metal Alloy for Metal Ceramic Restoration Use Brightis (Oct. 2011)
Vol. 11 Physical Properties and Safety of the Dental Adhesive, Multi Primer (Mar. 2014)

Vol. 12 Safety of the Dental Pulp Capping Material, TMR-MTA CEMENT ( Jan. 2018)《Previously Published Macromolecule Technology Reports》
Vol. 1 The Polymerization of Dental Materials: The Basis of Radical Polymerization (1) (Oct. 2009)Vol. 2 The Polymerization of Dental Materials: The Basis of Radical Polymerization (2) (Feb. 2010)
Vol. 3 The Polymerization of Dental Materials: Restoration-Material Monomers (1) (Mar. 2010)
Vol. 4 The Polymerization of Dental Materials: Restoration-Material Monomers (2) ( Jul. 2010)
Vol. 5 The Polymerization of Dental Materials: The Influence of Oxygen (Aug. 2011)
Vol. 6 The Polymerization of Dental Materials: Primers and Developers (Oct. 2012)

Vol. 7 Polymerization Silane Coupling Agent: Methacrylic Resin (Acrylic Resin) ( Jun. 2013)
Vol. 8 Shrinkage of Dental Composite in Polymerization (Nov. 2014)

Vol. 9 Application of Iodonium Salt as Initiator Component in Dental Material (Mar. 2017)
Vol.10 Application of Nanogel to Dental Resin and Adhesive ( Jun. 2018)《All Previously Published Science Reports》
Vol. 1 Dental Surgery and Bisphosphonate Formulation (Aug. 2010)

Vol. 2 Reactive Oxygen: Its Generation, Elimination and Effects (Nov. 2011)
Vol. 3 The Hypoxic World ( Jul. 2012)

Vol. 4 Recent Progress in the Regeneration of Tooth Material (Feb. 2014)
Vol. 5 Application of Fluoride and Its Effect (Oct. 2016)《Previously Published Product Reports》
Basic Information and Product Report on Zirconia (Feb. 2014)
Basic Information and Product Report on Titanium ( Jun. 2016)
Basic Information and Product Report on Hybrid Resin for CAD/CAM use (Sep. 2014)
Basic Information and Product Report on Dental Restorative Material (Sep. 2015)
Basic Information and Product Report on Dental Bonding Material ( Jan. 2016)
Product Report on Multi Primer Series (Oct. 2017)
KZR-CAD HR Block3 GAMMATHETA Product Report ( Jan. 2018)
Multi Etchant Product Report ( Jul. 2018)
Basic Information and Product Report on KZR-CAD NANOZR ( Jul.2018)

Editor: Takahiro Kato
Publisher: Shigenari Yamamoto
Date of publication: 5 Mar. 2019